Treatment of materials containing silk.



-' To all whom it'may concern:

I raw silk in order to V mainder.

the art, and

UNITED STATES PATENT OFFICE.

THEODORE IBOETTGER, OFI-IACKENSACK, AND FREDERICK PARK, NEW J'ERSEY; SAID 935,292. No Drawing.

v Be it known that WG,VTHEODORE BOETTGER and Fnnnnmcn VoM EYsER,'citizens of the United States, the said THEODORE BOE'I'IGER residing at Hackensack, Bergen county, New

Jersey, and the said Fnnomuon VOM EYSER residing at Rochelle Park, Bergen county, New Jersey, have invented certain new and useful Improvementsin the Treatment of Materials Containing Silk, of which the following is a specification.

Our invention relates to. the treatment of materials composed wholly or in part of prepare it for subseand other operations usual in its novelty consists in the manner in which the materials are treated and the reagents employed in the treatment.

Raw silk consists chiefly of two substances: The true silkfiber which is' called fibroin,. and which comprises about twothirds or more of its substance, and an outer layer, or covering, of a material called in the art hast and scientifically known as sericin, which makes up the bulk of the reg It also contains a very small amount' of wax, fat, coloring matter and quent dyeing ash. Most of the coloring matter is in theouter sericin layer. Sericin is a substance much resembling gelatin in its properties and is soluble in water only by prolonged boiling. Fibroin is a proteid and is not noticeably affected by proton ed boilin in water, but is somewhat read' y attacke by caustic alkalies, even in weak solutions, their action rendering it more" brittle and rough and diminishing its gloss. Fibroin is also attacked by soap solution, if it is boiled for a long time therein, but it is not acted upon by weak acid solutions.

In the preparation of silk for the dye bath, it has been customary to first treat it in a manner which is termed bo' of which consists in boiling it in a bath of soap and water, sometimes with the addition of carbonate of soda. The purpose of this treatment by boiling off is to remove the outer layer of sericin whereby the silk becomes lighter in COIOPf SiDCG most of the coloring matter is contained in the sericin layer,

and the luster is developed and it becomes Specification of Letters Patent.

Application filed November 20, 1908.

I terial whatever dust TREATMENT OF MATERIALS CONTAINING SILK.

Patented Sept. 28, 1909. Serial No. 463,567.

then dissolves leaving the lustrous and internal thread exposed. In treatin piece goods, which are composed in part 0% cotton or wool, the boiling ofi process serves the further purpose of cleansing from the mamay be adhering there- VOM EYSER, OF ROCHELLE VOM EYSEE ASSIGNOR TO SAID B OETT GER.

to and it tends also to improve the quality of the cotton or wool mixture. It 1s also customary to put the goods through a washing process after boiling off.

The boiling off and washing process consume much time and labor and employ materials which, while not-expensive 1n themselves or in small quantities, become expensive when used in large quantities as they must be used in the customary practice of the art.

The purpose of our invention is practically to eliminate the boiling off and washing process. Tov that end we treat the materials with a solution, in a novel way and with the result that not only is an enormous economy efiected but the goods are stronger, they are less liable to injury in the subsequent treatment to which they are subjected, they dye more rapidly, the finished product has a better appearance and they can be stripped after dyeing without deterioration in quality.

We first prepare our solution which consists essentially of a sulfated organic oil, water and an alkaline reagent suificient in. quantity to render the liquid alkaline in reaction but insuflicient injuriously to affect the fibrous material of the goods. By sulfated organic oil we mean an animal or vegetable oil, for instance, castor oil, which has been subjected to the action of sulfuric acid within certain limited ranges of temperature Washed with a salt solution and then treated with an alkali partly to neutralize the acid reaction. The object of this treatment is to render the oil miscible in'water. A good example of such a sulfated organic Oil is the liquid called Turkey red oil. A certain amount of unchanged oil and salts of the v fatty acids of the oil and various derivatives of the constituents of the oil are formed in the course of the treatment outlined and are to be found with the oil. This oil and others of the same class produced in substantially the same way, are not suitable for our purpose. They are usually acid in reaction to litmus even after the addition of a small portion of an alkali. 'In the preparation of our solution we add to 1 liter sodium ammonium phosphate less efiicient of water, about .7 5 cc. of the sulfated organic yet. Ammonia alone might be used, but a oil, .075 cc. of ammonia and from .75 to 1.5 comparatively large proportion would be rammes of sodium carbonate Of course it necessary. It is preferable to use an alka- 5 will be understood that these proportions line salt of an oxygenated acid because its 70 are relative. They are those which we preaction is moderate and. it does not disasfer in the light of our present knowledge. trously affect the fibroin.-

This solution it will be noted is in effect a Of course, it will be understood that if, weak solution slightly alkaline in character on account of previous or subsequent operaof the sulfated oil in water. It comprises tions in the treatment of the silk, the substi- 75 substantially one part of the oil to 1300' tution of other alkaline reagents for the parts of water. The proportion of water sodium carbonate is deemed desirable, then may be decreased possibly to 200 parts withthe precise quantities to be employed and out essentially varying the process but such the time during which the material should concentration is not necessary and when we be subjected to their influence, must in each so say a weak solution wemean one inwhich instance be determined by previous experithe water is present in a greater proportion m'ent, in a manner well known to those than 200 parts and yet one strong enough skilled in the art. After treatment with this to accomplish our purpose. Persons skilled solution the materials are ready immediately in the art will readily understand the limits for the dyeing operation and can be placed 85 ofeconomy and efliciency for any particular in the dye bath without washing.

kind of oil and alkali. Assuming this solu- If the exigencies of manufacture are such tion to have been prepared with the ingrethatthe materials are wholly or partly dried dients in the proportion stated, the raw silk after treatment in our novel solution then 5 or mixed goods is passed through the bath, it is sometimes preferable for instance, when which is previously brought to a temperaskein oods are treated, to wet them out beture of not quite 100 C. and are allowed to fore yeing. Under other circumstances remain in contact with the solution for a however, for instance, with mixed silk 3.1K space of abouttwenty minutes. cotton goods, they maybe wholly dried and- The sulfated oil seems to impart a high dyed without wetting or washing. As an 95 capillarity to the materials treated causmg example including the step of dyeing, we will the liquid to penetrate the fibers thoroughly describe the dyeing of Canton floss a light and efficiently. The solution also seems to blue color. The'silk is placed on sticks in have unusual and superior dissolving and usual manner and kept moving in a bath 'emulsifying properties. The weak alkaline consisting of 4 100 substance seems to act primarily as a hydro- Water 1000. 00 parts. lyzmg agent upon the sericin and incident- Turkey red 0il 1.00 ally it seems to increase the solvent power of Ammonia 10 the solution. The solution seems moreover Soda Ash 1.00

40 to be very mild in its action upon the fibroin at a temperature of about 99 degrees centi- 105 and leaves it coated with a very thin layer of rade (just below a simmer), till the desired mtrogeneous material which is repellant to egree of de g is attained (in P 1 water, though soluble, on prolonged boiling tice about 70 minutes It is then wrung, therein, or if an alkaline reagent is added Wet out, immersed, an moved in abath thereto. This layer probably protects the sisting of water 750 parts, spent liquor from 110 fi bro1n from weakening), not only during the the boiling off operation 250 parts, which time that it is in the ath, but also during has been made 'slightl acid by the addition 1 the subsequent operation of dyeing. This of a little sulfuric aci and xylene blue 1/10 later 18 removed in great measure during part, and kept moving till the shade is,-evenv the subsequent treatment of the goods. and of the desired intensity. (About35 115 F1brom coated with such a thin layer of minutes). It is then taken out, slightly ser1c1n, we believe to be an entirely novel scoured and finished with alittle soda-olive product or composition of matter. oil emulsion. The temperature of th e dge It will be under tood that other weak bath is about 80 degrees centigrade. f

alkahne substancesmay be used in place of course the details of the operation may be 20 sodium carbonate in connection with the su1'- 'widely varied without departing from the fated oil, and that such substances must be invention. v used in a quantity suflicient to, render the What we claim as new is:-- solution alkaline in reaction. The rate of 1. The process of treating material con removal of the sericin seems to vary with taining silk which consists in subjectin it 1 5 different alkaline reagents. Of the subto the action of a hot weak slightly alkaline stance which we have tested, for instance, solution of sulfated oil in water. borax, wasfound to be quite efiicient. Di- 2. The process of treating silk which con sodium hydrophosphate is less efficient than sists in subjecting it to, the-action 3f a \the borax if used inequal amount and dilweakly alkaline solution ofsulfated oil in sists in subjecting it heating the solution and the Sllk to a temperature not exceeding that of boiling water.

The process of treating silk, which con-- to the action of a Weakly alkaline solution of Turkey red oil 111 a relatively large quantity of hot Water.

4. The process of treating silk which consists in subjecting'it to the action of a weak solution of Turkey red oil in Water rendered slightly alkaline by the addition of an alkaline salt of an oxygenated acid.

A process-of dyeing materials containing silk which consists in subjecting them to the action a hot weak alkaline solution of sulfated oil in Water and subsequently placing them in a dye bath Without washing.

6. A process of dyeing materials containing sill which consists in subjecting them to the acti n of a hot Weak alkaline solution of sulfated oil in water, drying the material I and subsequently without washing.

7. A process of dyeing materials containing silk which consists in subjecting them to the action of a hot weak alkaline solution of sulfated oil in water, drying the materials, wetting them with water and then placing them in a dye hath without washing.

S. A process of dyeing materials containing silk which consists in subjecting them to the action of a hot weak alkaline solution of sulfated oil in water, removing them from the solution, wetting them out with water and then placing them in a dye bath without washing.

lVitness our hands this 18th day of November 1908, at New York, N. Y.

THEODORE BOETTGER. FREDERICH VOM ICYSER. lVitnesses:

I'IERMAN MEYER, lVILLIAM R. Bamm placing them in a dye bath 

